New Trends in Trace Elemental Analysis Elsamoul Hamdnalla Thermo Fisher Scientific The world leader in serving science
Introduction During the past decade ICPMS has developed from a delicate research tool, intended for the well-trained scientist only, into A more robust and well-established analytical technique for trace and ultra-trace element determination. ICPMS also shows a number of important limitations: The occurrence of spectral interferences. No information on the ‘chemical form’ Solid samples have to be taken into solution prior to analysis 2
Challenges. • For the analyst Sample Matrix Isobaric and polyatomic interference interference For The Operation. software simplicity Design Speciation 3
ICP-MS Performance for All Applications Thermo Scientific TM NEPTUNE Plus TM MC- ICP-MS Multicollector ICP-MS Thermo Scientific TM ELEMENT TM 2/XR HR-ICP-MS High Resolution ICP-MS Thermo Scientific TM iCAP TM TQ ICP-MS Triple quadrupole ICP-MS Thermo Scientific TM iCAP TM RQ ICP-MS Single quadrupole ICP-MS 4 4
Redefining Trace Element Analysis -Triple Quadrupole ICPMS All the Power, None of the Complexity Triple quadrupole accuracy with single quadrupole ease of use Q3 Robust design for routine analysis Advanced interference removal Q2 Flexible for advanced applications Integrated automation options Q1 Unique ease of use 5 5
Inside TQ Technology Quick-connect, self-aligning sample introduction system, Drop-down door for easy interface access. Q3 Range of interfaces provide full instrument flexibility, from maximum robustness to highest sensitivity. Q2 Zero user maintenance beyond the interface. Q1 Highest data accuracy in complex samples with the combined QCell and TQ functionality. 6
Applications We Are Going to Focus on... Environmental Analysis Clinical Research - Ti – As, Se Advanced Applications Metallurgy Speciation Analysis Nanoparticles 7
Redefining Trace Element Analysis -Triple Quadrupole ICPMS Meeting human health Advancing development and environmental in metals, materials and challenges chemicals • Clinical Research and Toxicology • Material Analysis • Metallopharmaceuticals • Nanoparticle Characterization • Environmental Analysis/Monitoring • Metallurgy • Food Safety • Energy Production 8 8
Determination of Trace Elements in Biological Samples • Trace Elements play important roles for correct funtion of living beings IntentionalExposure: Environmental Exposure: e.g. orthopedic surgery, drug treatment e.g. occupational health, work safety Matrix Characteristics Sample Preparation Urine Easy and pain-free to obtain Simple; Dilution High salt content Blood Contains protein bound metals Difficult; Microwave assisted digestion Viscosity, Precipitation Serum Reveals metal distribution in the bloodstream Simple; Dilution Salts, low molecular weightspecies 9 9
Analysis of Ti in Serum Product Ion 114 [Ti(NH 3 ) 3 NH] + •Ti may be released into the blood stream following degradation of 48 Ca + , 96 Zr ++ , 32 S 16 O + , + orthopedic or dental implants 31 P 16 O 1 H + , 24 Mg 2 Q3 isolates ions required • Low concentrations (less than for measurement (e.g. set to product ion 1 ng·mL -1 ) mass for Ti + at m/z 114) • Isobaric interference of main isotope 48 Ti through 48 Ca • PO + , POH + , CaH + interferences Q2 pressurized with reactive 48 Ti + 114 [Ti(NH 3 ) 3 NH] + gas to selectively generate on other Ti isotopes reaction products (e.g. NH 3 + Ti + Ti(NH 3 ) 3 NH + ) • Analytical methods need to be 114 Cd + , 98 Mo 16 O + Q1 set to analyte mass (e.g. Ti + at m/z 48) to Robust to cope with sample matrix filter out unwanted ions Sensitive to enable detection of low levels Specific to address Ti accurately despite interferences Analyte 48 Ti + 1 0 10
Solution – use the iCAP TQ Control ions entering the cell using Q1 • Use O to efficiently convert As and Se • 2 to AsO and SeO in Q 2 – the REE ++ don‘t react Selectively detect AsO and SeO free • from REE ++ interference, using Q 3 75 Method 78 Method Type As Se to to remove remove Polyatomic 40 Ar 35 Cl KED 40 Ar 38 Ar KED, H 2 40 Ca 35 Cl Isobaric 150 Nd 2 + O 156 Gd 2 + O 2 2 150 Sm 2+ 156 Dy 2 + ICP-MS using triple quadrupole technology – Thermo Scientific iCAP TQ ICP-MS 11
As and Se with REE Present - Results in Different Modes 1ppm Dy, Gd, Nd, Sm and Tb added • Interference removal capability • SQ- Increased BECs observed for all • modes due to unresolved doubly charged REE interferences Hydrogen is suitable for removing Ar • based polyatomics, but is not capable of fully removing REE 2 + interferences dramatically lower TQ - O mode shows • 2 BEC values for both As and Se 12
Proving the Accuracy of the Sample Analysis Sample analysis results Spike recovery in REE matrix solution Spike recovery results in (1 ppb As and Se) samples (1 ppb As and Se) Analyte AGV-1 Sediment Arsenic 94.6 % 97.6 % Selenium 93.4 % 97.6 % 13
Recovery of Ti in Serum using Different Measurement Modes Measured Ti Concentration in Ca-rich Blood Serum Samples Ti TQ-NH3 Ti SQ-NH3 Ti SQ-KED Reference Value 1 10 100 1000 10000 Ti Concentration (µg · L -1 ) 1 4 14
Recovery of Ti in Serum using Different Measurement Modes Measured Ti Concentration in Ca-rich Blood Serum Samples Ti TQ-NH3 Ti SQ-NH3 Single Quadrupole ICP-MS False positive results due to unresolved isobaric 48 Ca Interference! Ti SQ-KED Reference Value 1 10 100 1000 10000 Ti Concentration (µg · L -1 ) 1 5 15
Recovery of Ti in Serum using Different Measurement Modes Measured Ti Concentration in Ca-rich Blood Serum Samples Triple Quadrupole ICP-MS Only by using triple quadtechnology Ti TQ-NH3 can accurate results for Ti be obtained! Ti SQ-NH3 Ti SQ-KED Reference Value 1 10 100 1000 10000 Ti Concentration (µg · L -1 ) 1 6 16
Accurate Multielemental Analysis with TQ-ICP-MS • In Biological Samples • In Metals and Alloys • High detection sensitivity allows • Q1 separation of lower mass ions detection of low Titanium enables effective and complete concentrations in complex removal of all interferences on biological samples Selenium in Nickel alloys • Excellent agreement with certified • Only triple quadrupole ICP-MS is value obtained for Titanium in capable of fully resolving all spectral serum interferences • Full flexibility and usability of both single and triple quadrupole modes • Full multielemental analysis with dedicated interference removal for difficult analytes and comprehensive He KED in one run 17
Redefining TQ-ICP-MS with Unique Ease of Use Analyte Gas M + Product ion Result 18
Redefining TQ-ICP-MS with Unique Ease of Use 19
Advanced Applications using the iCAP TQ ICP-MS Speciation Analysis • control ChromControl plug-in for hardware • Hyphenation of Gas Chromatography (GC ) • using GCI-100 Analyte Advantage when using iCAP TQ Application S, P Improved Interference Removal, lower Speciation of Biomolecules background like proteins, peptides or DNA As Higher Sensitivity when analysing 75 As 16 O All sample matrices: instead of 75 As [KED] Food, Water, Urine etc. Se Higher Sensitivity when analysing SeO instead All sample matrices of Se [KED]; Reduced background on 80 Se 20
Advanced Applications using the iCAP TQ ICP-MS Nanoparticle Analysis • npQuant plug-in for Qtegra ISDS • Analyte Advantage when using iCAP TQ Application Au, Ag No apparent advantage High Detection Method Development, Sensitivity Validation Ti Increased specificity and lower background Environmental samples, Cosmetic products Others Improved interference removal is advantageous to reduce background and address particles more efficiently 21
iCAP TQ ICP-MS Application and Technical Notes Pharma Environment Metallurgy Clinical research Proof data for you to use 22
Which One Is Safer to Eat? What is the Speciation Analysis? Is the analytical activity of identifying and/ or measuring the quantities of one or more individual chemical species in a sample. CH 3 | As HO-As-OH As O H 3 C-As + -CH 2 CH 2 OH As | As || | OH As H 3 C-As-CH 3 CH 3 As | OH Total As concentration is not enough 23
Who Needs to Performs Speciation Analysis? Industries Applications • Hexavalent chromium, arsenic and bromate Environmental in drinking waters • Arsenic in fruit juices and rice grains Food Safety • Mercury in fish Occupational Exposure and • Hexavalent chromium in toy materials Consumer Goods Pharmaceutical • Mercury in herbal supplements Petrochemical • Sulfur/selenium in produced water 24
Regulations More regulations to come with ongoing assessments 25
How Do You Perform Speciation Analysis? Separation Detection Thermo Scientific ™ Dionex ™ ICS-5000 + HPIC ™ System Thermo Scientific TM iCAP Q ICP-MS System 26
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